CN101629019B - Basic biomass synthetic resin and preparation method and application thereof - Google Patents
Basic biomass synthetic resin and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the material science field, in particular to a basic biomass synthetic resin and a preparation method and an application thereof. The basic biomass synthetic resin is prepared by the following steps: taking acidity regulator to prepare a water solution with pH value of 6.0-10.0, adding plant protein powder in the water solution under the stirring state; adding a molecular structure modifying agent under the stirring state, performing the modifying reaction for 15-240 min at 5-75 DEG C; sequentially adding modified starch and a resin assistant, performing the polymerization reaction for 15-240min at 5-90 DEG C, adding preservative in a reaction system within the last 5-20min of the polymerization reaction; adding or not adding packing after finishing the reaction, and stirring uniformly to obtain the basic biomass synthetic resin, wherein the part of the materials is taken by weight. The basic biomass synthetic resin has wide application range on the respect of preparing bonding adhesive or coating.
Description
(1) technical field
The invention belongs to material science, particularly a kind of basic biomass synthetic resin and its production and application.
(2) background technology
The class that is meant biomass synthetic resin mainly adopts physics or chemical means that natural macromolecular such as protein, starch or carbohydrate are carried out appropriate modification, make it to possess some characteristic of synthetic resins, can replace traditional synthetic resins in certain Application Areas, the novel biomass synthetic materials that has complete nuisanceless degraded characteristics again simultaneously.
The composition principle of biomass synthetic resin mainly is that to adopt gentle chemical reagent or zymin in the reaction system that is solvent be simple chain structure with the natural macromolecular conformation transition of complexity with water, make and be hidden in intramolecular chemical functional group originally and come out, participate in intermolecular chemical reaction under certain condition, generate the polymkeric substance of body formula resin structure.
The Application Areas of biomass synthetic resin mainly contains aspects such as biomass adhesive, coating.
Biomass adhesive has degradable, free of contamination advantage, and since last century the '30s, in wood processing field, people make great efforts to take the whole bag of tricks to make biomass adhesive enter large-scale industrial production always.In early stage, be that the biomass adhesive of representative had once occupied 85% of U.S. glued board market with the rubber made from soybean cake.But after World War II,, be that the tackiness agent of base-material has replaced the rubber made from soybean cake stick gradually with the petroleum derivative along with the development of petroleum industry.Synthetic adhesive is more cheap, and better bonding strength and water resisting property are arranged.The synthetic adhesive that with " three-aldehyde glue " is representative occupy dominant position for a long time in the wood-based plate field.Although the various countries scientist takes various ways that biological material is carried out modification, up to the present, still there is big gap in biomass adhesive with adhesive made of synthetic resin on using.
Utilize the protein modified making wood adhesive of soybean or other plant, many bibliographical informations have been arranged, and (USPatent 6306997, Soybean-based adhesive resins and composite productsutilizing such adhesives; US Patent 6497760, Modified soy proteinadhesives; Enzhi C., Xiuzhi S., Greggory S.Karr, Adhesive properties ofmodified soybean flour in wheatstraw particleboard, Composites, Part A35,2004,297302; Rakesh K., Veena C., Saroj M., Adhesives and plasticsbased on soy protein products, Industrial Crops and Products, Volume 16, and Issue 3, and November 2002,155-172; Chinese patent 200410002616.9 " a kind of soybean source tackiness agent and preparation method thereof ").Utilize starch denaturalization to make the method for tackiness agent, can reference United States Patent 3836376, Starch-based adhesive compositions; United States Patent 5181959, High-concentration starch adhesive.
Aspect the research that utilizes biological material making coating, main research emphasis is to utilize starch or modified starch to substitute a part of synthetic materials as supplementary material to be applied in the water-borne coatings.Relevant patent is seen Chinese patent ZL99119229.x, ZL93106278.0 and ZL200710143428.1, the correlative study article is seen " application of starch in coating ", and (numb filial piety is brave, the Anhui chemical industry, 2007 (01)), " starch-phenylethene grafted copolymer is done the research of waterproof paint " (Duan Xiangzhi etc., Xinyang Normal College's journal (natural science edition), 1997 (04)) etc.
Comprehensive achievement in research both at home and abroad, the subject matter that reflects is to lack the macromole characteristic of natural biological material and chemical functional group's full appreciation, the purpose and the purposes of modification are single, cause product application to have more serious defective, do not possess the base attribute as basic material.
(3) summary of the invention
The object of the invention is to provide a kind of basic biomass synthetic resin, and it has the base attribute of basic material, applied range.
The technical solution used in the present invention is as follows:
Basic biomass synthetic resin makes as follows: get 0.1～15 part of acidity regulator and be mixed with the aqueous solution that pH is 6.0-10.0, add 5～20 parts of plant protein powders under the whipped state and control pH value of solution at 6.0-10.0 in solution; Keep whipped state to add 0.05～20 part of molecular structure properties-correcting agent down, carry out modified-reaction 15～240min in 5～75 ℃; Add 0～10 portion of modified starch, 0.05～40 part of resin additive successively, polyreaction 15～240min under 5～90 ℃ of conditions; At the last 5～20min of polyreaction, in reaction system, add 0.1～10 portion of sanitas; After reaction finishes, add 0～20 part of filler and stir and promptly obtain basic biomass synthetic resin, each material umber is a weight part.
Protein content in the described plant protein powder is not less than 50wt%.
Described plant protein powder is one or more the combination in defatted soyflour, soybean protein isolate, soybean protein concentrate, degreasing Zein powder, degreased peanut flour, gluten powder, degreasing rapeseed meal, the degreasing cottonseed meal.
Described acidity regulator is one or more the combination in citric acid, Trisodium Citrate, yellow soda ash, water glass, sodium bicarbonate, sodium-acetate, SODIUM PHOSPHATE, MONOBASIC, Sodium phosphate dibasic, boric acid, oxalic acid, hydrochloric acid, sulfuric acid, sodium hydroxide, potassium hydroxide, the Seignette salt.
Described molecular structure properties-correcting agent be phosphorus oxychloride, diacetyl oxide, succinyl oxide, hexanodioic acid, oxalic dialdehyde, one or more combination in the glutaraldehyde, sodium laurylsulfonate, Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, sodium bisulfite, S-WAT, Potassium hydrogen sulfite, ammonium sulphite, ammonium bisulfite, trypsinase, trans-glutaminases, lauric acid, mercaptoethanol, Thiovanic acid, sulfo-threitol, urea, Guanidinium hydrochloride.
Described modified starch is one or more the combination in starch bisphosphate, starch acetate, hydroxypropylated starch, hydroxyethylamyle, carboxymethyl starch, cross-linking starch, cationic starch, the Sumstar 190.
Described resin additive is one or more the combination in tetracol phenixin, normal hexane, triphenylphosphate, tributyl phosphate, mono-glycerides, Resorcinol, Resorcinol, pyrocatechol, glycerine, sorbyl alcohol, ethylene glycol, glycol ether, seaweed gel, guar gum, xanthan gum, gum arabic, polyoxyethylene, polyvinylpyrrolidone, polyvinyl alcohol, sodium polyacrylate, the polyacrylamide.
Described sanitas be potassium sorbate, phytic acid, dehydroacetic acid (DHA), butyl p-hydroxybenzoate, Imidurea, diazonium Imidurea, isothiazolinone, 10,10 '-one or more combination in the oxo Shuan Fen Evil arsenic, dimethyl fumarate, sodium Diacetate, Sodium Benzoate, Sodium Propionate, calcium propionate.
Described filler is one or more the combination in flour, diatomite, kaolin, wilkinite, lime carbonate, silicon-dioxide, potter's clay, wollastonite, ground barium sulfate, the Mierocrystalline cellulose.
The temperature of described modified-reaction is: being 15 ℃～60 ℃ during acylation modification, is 15 ℃～45 ℃ during esterification modification, and surfactant-modified or reduction is 20 ℃～60 ℃ during modification, is 5 ℃～50 ℃ during the urea modification, is 25～50 ℃ during enzyme-modified.
Basic biomass synthetic resin provided by the present invention is the primary products of biomass synthetic resin, is the mixture of chain type and body formula structure.Because its characteristics of molecular structure, basic biomass synthetic resin has shown some special propertys, as has special flowing law, good film-forming properties, stickiness, powder reduction characteristic and hydrophilic materials such as timber, body of wall are had good adhering to and adhesion properties etc.These character are indicating that all basic biomass synthetic resin has the potential use as wood adhesive, coating and plasticity-powdered material.
The present invention has following advantage with respect to prior art:
(1) basic biomass synthetic resin of the present invention is as product structurally-modified to natural macromolecular and reorganization, held the macromolecular chemical structure characteristic of natural biological comprehensively, under the prerequisite of the inner covalent linkage of saboteur not, realized effective transformation of molecular function.Reaching on the purpose basis of specific function, the energy that expends in the production process greatly reduces than the crosslinked again again method of complete degradation biological matter macromole, has realized making full use of of the resource and the energy, and production process is environment friendly and pollution-free.
(2) basic biomass synthetic resin is a kind of brand-new material system, shows and existing tackiness agent and all different characteristic of coating system, mainly shows as non-Newtonianism fluidic characteristic on flowability; During envrionment temperature-10～40 ℃, system viscosity changes between 2500～8000cps, and the major function characteristic is unaffected; Have the water of adding reduction characteristic etc. after being dried to powder, above characteristic has determined the extensive use of basic biomass synthetic resin aspect wood adhesive, coating and resin-oatmeal.The wood adhesive of basic biomass synthetic resin preparation has easy, the bonding strength advantages of higher of application, be applied to the glued board series products, bonding strength mean value is (GB/T9846-2004 regulation 〉=0.70Mpa is salable product) more than 1.0Mpa, and sheet material does not have obnoxious flavour releases such as formaldehyde substantially.
(3) because water is good solvent of biomass synthetic resin and softening agent, therefore after the basic biomass resin-oatmeal being added a certain amount of water and mixing, can reduce dehydrate before every basic function of resin solution.Simplify application, storage and the transportation of basic biomass synthetic resin, expanded the application space.
(4) embodiment:
Below with specific embodiment technical scheme of the present invention is described, but protection scope of the present invention is not limited thereto:
Embodiment 1
Basic biomass synthetic resin, its parts by weight of raw materials consists of:
Defatted soyflour 10
Water 100
Yellow soda ash 0.2
Diacetyl oxide 1
Dialdehyde starch 5
Resorcinol 0.1
Sodium polyacrylate 0.1
Dehydroacetic acid (DHA) 0.25
Nano silicon 5
Preparation process is: in reactor, yellow soda ash is dissolved in the water to be made into pH value be 9.0 solution, and is preheated to 40 ℃, get load weighted defatted soyflour and slowly add, adopt 150 rev/mins rotating speed to stir and control pH value in adition process; After stirring becomes the homogeneous emulsion, diacetyl oxide divided add for 5 times in the reaction system, 10min adds and finishes.Stirring velocity is reduced to 75 rev/mins, insulation reaction 60min.Progressively raise temperature of reaction system to 90 ℃, add dialdehyde starch and Resorcinol this moment successively, carries out the resin polymerization reaction.When reaction proceeds to 60min, add sodium polyacrylate, continue reaction 20min.10min before reaction finishes adds dehydroacetic acid (DHA); Reaction is cooled to 25 ± 5 ℃ after finishing, and adds nano silicon, continues to stir 5min and gets product.
Embodiment 2
Basic biomass synthetic resin, its parts by weight of raw materials is composed as follows:
Degreasing cottonseed meal 9
Water 100
Sodium-acetate 5
Sodium phosphate dibasic 5
Trypsinase 60U
Trans-glutaminases 45U
Starch bisphosphate 3
Glycol ether 1
Seaweed gel 0.3
Dimethyl fumarate 0.5
Preparation process is: in reactor, sodium-acetate and Sodium phosphate dibasic are made into pH8.0 buffered soln in proportion.Under 30 ℃ of conditions, in buffered soln, slowly add degreasing cottonseed meal, 90 rev/mins of mixing speed.Keep mixing speed constant, add trypsinase, reaction 60min; Be warming up to 40 ℃ gradually and add trans-glutaminases, insulation reaction 30min.The first step reaction finishes, and adds starch bisphosphate, seaweed gel successively, and the system temperature of reaction is increased to 80 ℃, carries out the resin polymerization reaction, stirs 30min, adds glycol ether, continues reaction 30min, and 5min before reaction finishes adds dimethyl fumarate.Reaction is cooled to 25 ℃ with system temperature after finishing, and gets product.
Embodiment 3
Basic biomass synthetic resin, its parts by weight of raw materials is composed as follows:
Degreased peanut flour 15
Water 100
Oxalic acid 0.3
Potassium hydroxide 0.06
Ammonium sulphite 0.2
Succinyl oxide 0.3
Hexanodioic acid 0.2
Sumstar 190 5
Xanthan gum 0.2
Diazonium Imidurea 0.1
Kaolin 10
Preparation process is: in reactor, oxalic acid and potassium hydroxide are made into pH9.0 buffered soln in proportion.Under 30 ℃ of conditions, in buffered soln, slowly add degreased peanut flour, 90 rev/mins of mixing speed.Keep mixing speed constant, add ammonium sulphite, insulation reaction 60min; Add hexanodioic acid, succinyl oxide successively, keep mixing speed, react 60min again; Add Sumstar 190, xanthan gum successively, the system temperature of reaction is increased to 85 ℃, carry out the resin polymerization reaction, stir 60min.10min before reaction finishes adds the diazonium Imidurea.After reaction finished, adding kaolin also stirred, and system temperature is cooled to 20 ℃, gets product.
Embodiment 4
Basic biomass synthetic resin, its parts by weight of raw materials is composed as follows:
Gluten powder 9
Water 100
Sodium bicarbonate 0.5
Sodium hydroxide 0.06
Mercaptoethanol 0.03
Guanidinium hydrochloride 0.6
Lauric acid 0.03
Pyrocatechol 0.01
Polyvinyl alcohol 0.1
Isothiazolinone 0.3
Preparation process is: in reactor, sodium bicarbonate and sodium hydroxide are made into pH9.5 buffered soln.Under 25 ℃ of conditions, in buffered soln, slowly add gluten powder.Add mercaptoethanol, reaction 25min adds Guanidinium hydrochloride, lauric acid more successively, continues reaction 50min; Add pyrocatechol, polyvinyl alcohol successively, the system temperature of reaction is increased to 60 ℃, carry out the resin polymerization reaction, stir 55min; 5min before reaction finishes adds isothiazolinone.Reaction is cooled to 25 ℃ with system temperature after finishing, and gets product.
Embodiment 5
Basic biomass synthetic resin, its parts by weight of raw materials is composed as follows:
Defatted soyflour 12
Water 100
Citric acid 0.3
Trisodium Citrate 0.6
Urea 3
Glutaraldehyde 0.05
Polyoxyethylene 0.03
Calcium propionate 0.25
Preparation process is: in reactor, citric acid and Trisodium Citrate are made into pH6.5 buffered soln.Under 30 ℃ of conditions, in buffered soln, slowly add defatted soyflour.Add urea, reaction 60min adds glutaraldehyde, keeps stirring and reacts 30min again; Add polyoxyethylene, the system temperature of reaction is increased to 65 ℃, carry out the resin polymerization reaction, stir 30min; 5min before reaction finishes adds calcium propionate.Reaction is cooled to 25 ℃ with system temperature after finishing, and gets product.
Application examples 1: basic biomass synthetic resin is applied to veneer plywood (HWPW-VC).
Basic biomass synthetic resin that embodiment 1 is obtained and lime carbonate mix standby with 100: 10 mass ratio.
The veneer moisture content of forming glued board is controlled at 12～15%.Long core direction is spliced into complete central layer; Again the complete central layer of the horizontally-spliced one-tenth of veneer of short core direction.
To concoct uniform resin compound on the roll-type spreadometer to the two-sided applying glue of short central layer after with the long central layer assembly formation plate base that superposes in length and breadth.
Under the pressure of 0.8Mpa, 60min colds pressing with the plate base; On thermocompressor, take the parameter of 120 ℃ of temperature, pressure 0.9Mpa to carry out hot pressing subsequently, after operations such as sanding and facing, obtain production board.
By the hardwood plywood bonding strength of the inventive method processing greater than 1.0MPa (GB/T9846-2004 is 〉=0.70MPa), burst size of methanal only 0.1mg/L (GB/T9846-2004 is≤0.5mg/L).
Application examples 2: with the basic biomass synthetic resin power applications in veneer plywood (HWPW-VC).
The basic biomass synthetic resin that embodiment 2 obtains is made toner by vacuum concentration and spraying drying operation.
Before using, toner and the mass ratio of water with 1: 3 are mixed, mixed system is the solution state of homogeneous at this moment.Again that this resin solution and lime carbonate is even with 100: 10 mass ratio blending.
Toner is applied directly to the veneer surface carries out hot pressing, 120 ℃ of hot pressing temperatures, pressure 1.0Mpa.
By the hardwood plywood bonding strength of the inventive method processing reach 1.0MPa (GB/T9846-2004 for 〉=0.70MPa), sheet material burst size of methanal 0.05mg/L (GB/T9846-2004 is≤0.5mg/L).
Application examples 3: basic biomass synthetic resin is applied to interior wall coating
It is 20% the aqueous solution that the basic biomass synthetic resin that embodiment 3 is obtained is mixed with mass concentration, with ground barium sulfate, lime carbonate, titanium dioxide with 100: 10: 5: 1 mass ratio mixes, in colloidal mill, further grind to form slurry, obtain the coating finished product.
This coating has that rate of drying is fast, and film-forming properties is stronger, inner wall of building is had characteristics such as good adhesive ability, water-fast washing and wet rubbing, and adding mineral pigment can the furnishing shades of colour, and indoor formaldehydeless and other obnoxious flavoures in dry back detect.
Claims (9)
1. basic biomass synthetic resin is characterized in that, makes as follows: get 0.1～15 part of acidity regulator and be mixed with the aqueous solution that pH is 6.0-10.0, add 5～20 parts of plant protein powders under the whipped state and control pH value of solution at 6.0-10.0 in solution; Keep whipped state to add 0.05～20 part of molecular structure properties-correcting agent down, carry out modified-reaction 15～240min in 5～75 ℃; Add 0～10 portion of modified starch, 0.05～40 part of resin additive successively, polyreaction 15～240min under 5～90 ℃ of conditions at the last 5～20min of polyreaction, adds 0.1～10 portion of sanitas in reaction system; After reaction finishes, add 0～20 part of filler and stir and promptly obtain basic biomass synthetic resin, each material umber is a weight part; Described described molecular structure properties-correcting agent be phosphorus oxychloride, diacetyl oxide, succinyl oxide, hexanodioic acid, oxalic dialdehyde, one or more combination in the glutaraldehyde, sodium laurylsulfonate, Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, sodium bisulfite, S-WAT, Potassium hydrogen sulfite, ammonium sulphite, ammonium bisulfite, trypsinase, trans-glutaminases, lauric acid, mercaptoethanol, Thiovanic acid, sulfo-threitol, urea, Guanidinium hydrochloride.
2. basic biomass synthetic resin as claimed in claim 1 is characterized in that the protein content in the described plant protein powder is not less than 50wt%.
3. basic biomass synthetic resin as claimed in claim 1, it is characterized in that described plant protein powder is one or more the combination in defatted soyflour, soybean protein isolate, soybean protein concentrate, degreasing Zein powder, degreased peanut flour, gluten powder, degreasing rapeseed meal, the degreasing cottonseed meal.
4. basic biomass synthetic resin as claimed in claim 1, it is characterized in that described acidity regulator is one or more the combination in citric acid, Trisodium Citrate, yellow soda ash, water glass, sodium bicarbonate, sodium-acetate, SODIUM PHOSPHATE, MONOBASIC, Sodium phosphate dibasic, boric acid, oxalic acid, hydrochloric acid, sulfuric acid, sodium hydroxide, potassium hydroxide, the Seignette salt.
5. basic biomass synthetic resin as claimed in claim 1, it is characterized in that described modified starch is one or more the combination in starch bisphosphate, starch acetate, hydroxypropylated starch, hydroxyethylamyle, carboxymethyl starch, cross-linking starch, cationic starch, the Sumstar 190; Described resin additive is one or more the combination in tetracol phenixin, normal hexane, triphenylphosphate, tributyl phosphate, mono-glycerides, Resorcinol, Resorcinol, pyrocatechol, glycerine, sorbyl alcohol, ethylene glycol, glycol ether, seaweed gel, guar gum, xanthan gum, gum arabic, polyoxyethylene, polyvinylpyrrolidone, polyvinyl alcohol, sodium polyacrylate, the polyacrylamide.
6. basic biomass synthetic resin as claimed in claim 1, it is characterized in that described sanitas is one or more the combination in potassium sorbate, phytic acid, dehydroacetic acid (DHA), butyl p-hydroxybenzoate, Imidurea, diazonium Imidurea, isothiazolinone, dimethyl fumarate, sodium Diacetate, Sodium Benzoate, Sodium Propionate, the calcium propionate; Described filler is one or more the combination in flour, diatomite, kaolin, wilkinite, lime carbonate, silicon-dioxide, potter's clay, wollastonite, ground barium sulfate, the Mierocrystalline cellulose.
7. basic biomass synthetic resin as claimed in claim 1; it is characterized in that; the temperature of described modified-reaction is: be 15 ℃～60 ℃ during acylation modification; be 15 ℃～45 ℃ during esterification modification; surfactant-modified or reduction is 20 ℃～60 ℃ during modification; being 5 ℃～50 ℃ during the urea modification, is 25～50 ℃ during enzyme-modified.
8. the preparation method of the described basic biomass synthetic resin of one of claim 1-7 is characterized in that step is as follows:
Get 0.1～15 part of acidity regulator and be mixed with the aqueous solution of pH value, in solution, add 5～20 parts of plant protein powders under the whipped state and control the pH value at 6.0-10.0 for 6.0-10.0; Keep whipped state to add 0.05～20 part of molecular structure properties-correcting agent down, carry out modified-reaction 15～240min in 5～75 ℃; Add 0～10 portion of modified starch, 0.05～40 part of resin additive successively, polyreaction 15～240min under 5～90 ℃ of conditions; At the last 5～20min of polyreaction, in reaction system, add 0.1～10 portion of sanitas; After reaction finishes, add 0～20 part of filler and stir and promptly obtain basic biomass synthetic resin, each material umber is a weight part.
9. the application of the described basic biomass synthetic resin of claim 1 aspect preparation tackiness agent or coating.
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